CN101146379B - Heater, apparatus, and associated method - Google Patents

Heater, apparatus, and associated method Download PDF

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Publication number
CN101146379B
CN101146379B CN2006100647892A CN200610064789A CN101146379B CN 101146379 B CN101146379 B CN 101146379B CN 2006100647892 A CN2006100647892 A CN 2006100647892A CN 200610064789 A CN200610064789 A CN 200610064789A CN 101146379 B CN101146379 B CN 101146379B
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Prior art keywords
pipe
heater
packing material
heating element
volume
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CN101146379A (en
Inventor
R·A·吉丁斯
M·P·德埃弗林
S·戴
B·J·巴丁
L·Q·曾
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Slt Technology Co
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General Electric Co
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24HFLUID HEATERS, e.g. WATER OR AIR HEATERS, HAVING HEAT-GENERATING MEANS, e.g. HEAT PUMPS, IN GENERAL
    • F24H7/00Storage heaters, i.e. heaters in which the energy is stored as heat in masses for subsequent release
    • F24H7/06Storage heaters, i.e. heaters in which the energy is stored as heat in masses for subsequent release the released heat being radiated
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/40Heating elements having the shape of rods or tubes
    • H05B3/42Heating elements having the shape of rods or tubes non-flexible
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24HFLUID HEATERS, e.g. WATER OR AIR HEATERS, HAVING HEAT-GENERATING MEANS, e.g. HEAT PUMPS, IN GENERAL
    • F24H7/00Storage heaters, i.e. heaters in which the energy is stored as heat in masses for subsequent release
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/40Heating elements having the shape of rods or tubes
    • H05B3/42Heating elements having the shape of rods or tubes non-flexible
    • H05B3/48Heating elements having the shape of rods or tubes non-flexible heating conductor embedded in insulating material
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/40Heating elements having the shape of rods or tubes
    • H05B3/42Heating elements having the shape of rods or tubes non-flexible
    • H05B3/48Heating elements having the shape of rods or tubes non-flexible heating conductor embedded in insulating material
    • H05B3/52Apparatus or processes for filling or compressing insulating material in tubes

Abstract

A heater that may include an outer housing and an inner tube is provided. The inner tube is in a coaxial relation to and within the outer housing. An inward facing surface of the inner tube defines a volume sufficient to receive a reaction capsule, and the outward facing surface is radially spaced from an inward facing surface of the outer housing sufficient to define a gap. A filler material is disposed within the gap. The filler material responds to pressure such that the filler volume is reduced by less than 5 volume percent at greater than 500 MPa pressure and at greater than 500 DEG C temperature. One or more heating elements are disposed in the gap. The heating elements are in thermal communication with the inner tube.

Description

Heater, device and correlation technique
Technical field
The present invention includes the embodiment of device of relating to heater, comprising this heater and associated method.
Background technology
High-pressure installation can be included in the heater of heated parts under the pressure.This heater can comprise one or more heating elements.The heating element that is applicable to gaseous pressure mediums may not be suitable for the solids pressure medium, and the solids pressure medium is subjected to radially outer pressure, rather than is subjected to the uniform pressure (for example being immersed in the hyperbaric environment) from all directions.That is to say that this heater can change volume under operating condition, but do not need to or transmit pressure from workpiece.The known heater that is used to have the high pressure chest of solids pressure medium, changing distortion in high-pressure high-temperature environment after, its volume/shape can only use once, and there is batch variation the disposable use unit of some prior aries, causes technique change between twice operation.
Need a kind of heater, be used for the heating element of this heater, and the device that comprises heater, this heater can be used in the high-pressure and high-temperature device, and volume is almost constant, allows to reuse.Also need to make and/or use heater, be used for the heating element of this heater and/or comprise the method for the high-pressure and high-temperature device of heater, this heater can use repeatedly.
Summary of the invention
The present invention includes the embodiment that relates to heater.Heater comprises first pipe that has defined central shaft, and this first pipe has first end and second end, and second end and the first end axially-spaced; Shell comprises at least one second pipe; The packing material setting wherein responds the pressure greater than 500MPa in the enclosure, and packing material can reduce less than 5 percents by volume on the volume under 500 ℃ the temperature being higher than.One or more heating elements are at least partially disposed in the packing material.The heating element and the first pipe thermal communication, first pipe is at least partially disposed in the shell or next-door neighbour's shell.The inner surface of first pipe can hold a container, and discharges this container after operation.
The present invention includes the embodiment that relates to heater, this heater comprises the housing with inner surface and outer surface.Inner surface defines the chamber that is configured for storage container, and outer surface defines groove or passage.Heating element is set in this groove or the passage.
The present invention includes the embodiment that relates to the method that forms this heater.This method comprises with solia particle filling base, reaches the density greater than 50 percents by volume; And the base of filling injected cement material.
The present invention includes the embodiment that relates to device.This device comprises heating element.This heating element is heated to the temperature range greater than 500 ℃; The cement charges of parcel heating element; First pipe communicates with the inner surface of cement charges, and also provides mechanical support, and second pipe, communicates with the outer surface of cement charges.In operation, the energy that offers heating element causes heat energy to flow into first pipe entering the container that is arranged in the territory, first area under control, this heat enough makes vessel temp be elevated to temperature range greater than 500 ℃, and as the response that temperature raises, the enough pressure that in container, produces greater than the scope of 500MPa.When this temperature and pressure raise generation, heater was with the second pipe mechanical support by the device balance, thereby restriction first pipe makes the interior volume increase of container less than 5%.
Description of drawings
Fig. 1 is the schematic diagram that shows the heater that comprises the embodiment of the invention.
Fig. 2 is a schematic diagram, has shown to comprise the device that can use the embodiment of the invention of heater among Fig. 1.
Fig. 3 is the schematic diagram that shows the heater that comprises the embodiment of the invention.
Fig. 4 is the schematic representation of apparatus according to the embodiment of the invention.
Embodiment
All scopes of specification and claim comprise that all the numerical value end points also can independent combination.Numerical value in specification and the claim is not limited to determined value, but may comprise the numerical value different with determined value.Numerical value is understood as that very thereby inaccuracy comprises the numerical value approaching with fixed value, the existence of the experimental error that the accuracy of use instrument causes when allowing owing to measuring technique known in the art and/or definite numerical value.
Scope and the end value determined in specification and the claim, for example, the scope and the end value of temperature, pressure, concentration etc. can make up and/or exchange, and be included as the subrange of reasonable subunit.
Here the approximate language that uses from the beginning to the end in specification and claim can be used for revising any quantificational expression, and only otherwise cause its basic function that relates to change, described quantificational expression allows to change." unconfined " can use in conjunction with term, also can comprise the digital or micro-of the imagination, also still is counted as not being subjected to improve simultaneously the constraint of term.Term " pitch " comprises the take up an official post distance of what some respective point to the adjacent coiling coil of coiling coil, measures by being parallel to longitudinal axis." can cast " and refer to by being filled into the ability of formation given shape in the mould.Term used herein " groove " comprises the elongated recess and/or the otch on the surface that is used for holding heating element, and wherein depression and/or otch have the shape of cross section that lacks the lower surface angle.Term used herein " passage " comprises the elongated recess and/or the otch on the surface that is used for holding heating element, and wherein depression and/or otch have the shape of cross section that comprises at least one lower surface angle.
Device according to the embodiment of the invention comprises housing, is arranged on the heater in the housing, and is arranged on the heating element in the heater.In one embodiment, housing comprises many pipes.In another embodiment, first pipe and second pipe are microscler, define central shaft respectively.When coaxial relative to each other setting, and first pipe is at least partially disposed in second pipe, and first and second pipes have common central shaft.Every Guan Douyou is towards the first surface in the outside with towards the second surface of inboard.The second surface of the first surface of first pipe and second pipe radially separates, to limit the annular space between the pipe.In one embodiment, one or two pipe is cylindrical shape and/or is made of metal.In other embodiments, one or more pipes can be polygons, for example hexagon or pentagon, and each limit all is irregular relative to each other.
Every pipe all has first end and second end.Second end and the first end axially-spaced.In one embodiment, end ring is welded on a pipe or two pipes, for example, and the one or both ends of every pipe.This ring defines the end of the annulus between first pipe and second pipe.In one embodiment, the shape of each ring is encircled the shape of one or two pipe of being fixed corresponding to this.For example, a columnar pipe has annular or discoidal end ring.This ring can be by predetermined tolerance by the machine manufacturing, and described predetermined tolerance minimizes the space between the corresponding contact zone on contact area on this ring and one or two tube-surfaces.Further, these rings go up to form one or more holes, thereby allow one or more metal wire etc. to pass through, and metal wire etc. pass this ring from annular space or slit and reach the surrounding environment.End ring can be fixed on the pipe end by welding, brazing or similar approach.In one embodiment, end ring is connected by screw thread jointly with pipe end.
The second surface of first pipe is by being designed size, formalizing and being configured to hold reaction vessel.Select suitable material and structure, make the processing back discharge container easily.In one embodiment, provide reusable heater, it can hold a plurality of reaction vessels continuously, and finishes reaction in each container.In certain embodiments, the root mean square of the surface roughness of first pipe is less than 1 millimeter (mm).In second embodiment, pipe does not have any slit, crack or the interruption of size greater than 5mm.
The example of the metal that pipe and/or ring adopt comprises ferrous alloy, for example steel.In other embodiments, pipe and ring end are made by cermet, pottery or composite material.In one embodiment, first and second pipes and corresponding end ring comprise the high temperature superalloy that one or more plastic deformations under operating condition are low relatively.Suitable superalloy comprises INCONEL 718 and HASTELLOY X, and they can (Magellan Industrial Trading Company Inc.) buys (Connecticut State, southern Norwalk) by Mai Zhelun industry commerce and trade Co., Ltd.
Heating element is arranged in the annular space between first and second pipes.In one embodiment, be full of packing material in the annular space, for example cement, and annular space comprises the one or more heating elements that are arranged in the grafting material.In one embodiment, it is that can cast or curable filling grafting material, fills grafting material like this and can be used as that fluid is poured or fill, and hardening becomes solid then.In one embodiment, grafting material has higher relatively density and/or lower porosity.In another embodiment, grafting material has higher relatively alumina content.Suitable grafting material helps in operation internal pressure to be delivered to second pipe from first pipe as the use in the annular space of filler between first and second pipes.
The creep of finishing part that the selection of suitable grafting material is based on compressive failure, further densification and/or is made by cement, described creep is left in the basket under operating conditions.In one embodiment, grafting material comprises the cement of the high alumina content that can cast.In second embodiment, its theoretical maximum density relatively, grafting material has the relative density greater than 75%.In the 3rd embodiment, the relative density of cement is selected from following scope: the 75-80% of the theoretical maximum density of relative bonding material, and 80-85%, 85-90%, 90-95%, and greater than 95%.
The nonrestrictive example of cement comprises aluminium oxide and magnesian mixture.In one embodiment, cement comprises the aluminium oxide that accounts for total amount 70-80% weight range.In one embodiment, cement comprises and accounts for the aluminium oxide of total amount greater than 50% weight range.In one embodiment, cement mainly is made up of aluminium oxide and gluing mixture thereof.In one embodiment, cement comprises the V family metal on aluminium oxide, magnesium and at least a periodic table of elements.In one embodiment, cement mainly is made up of aluminium oxide and magnesium oxide.In one embodiment, the solia particle that is used in the cement has face coat, and this has relatively increased wetting effect and reduced the space and has formed.Suitable cement, for example AREMCO 575N and AREMCO 576N can be bought (Valley Cottage, New York) by Aremco Product.
In one embodiment, under the working temperature of device, when compression pressure reached 1000 megapascal (MPa)s (Mpa), packing material can be resisted crushing, densification or both.In one embodiment, packing material response greater than the pressure of 500Mpa and be higher than 500 degrees centigrade (℃) temperature, the volume of packing material reduces less than 5vol.%.In one embodiment, heater uses in device, and the pressure limit of this device operation is selected by following any one scope: 10-50MPa, 50-100MPa, 100-150MPa, 150-250MPa, 250-300MPa, 300-400MPa, 400-500MPa, 500-600MPa, 600-700MPa, 700-800MPa, 800-900MPa, 900-1000MPa and greater than 1000MPa.In another embodiment, heater is applied under the temperature range of operation, and described scope is selected by following any one scope: 200-500 ℃, and 500-750 ℃, 750-1000 ℃, 1000-1250 ℃, 1250-1500 ℃ and greater than 1500 ℃.
In one embodiment, heater forms by base is filled to annular space, and this base is made up of microparticle material, and microparticle material comprises that high-alumina grinds pearl, or large scale (for example average diameter of 1.5mm) fusion-cast particle.According to the expection end structure of heating element in the base, heating element is provided with in the mode of determining.Base is by vibrating device and/or press filling.In one embodiment, base is filled to the relative density that has greater than 50 percents by volume (vol.%) by solia particle.Suitable oxidizing aqueous aluminium base cement is used to inject, immerse and/or penetrates into gap or the void space that is limited by pearl or particle.After grafting material solidified, consequent cement structure had appropriate density disclosed herein.This structure is full of the space between second and first metal tube, surrounds and support heating element.
In one embodiment, the cement of heater part can followingly form.Heater is partly assembled, thereby makes first and second pipes, heating element and an end ring be positioned at suitable position.Heater is erected at the end that opening makes progress, and solia particle is added into the shallow degree of depth.The definite degree of depth is by the ability decision of effectively cement being injected base and avoiding air pocket to form simultaneously.In certain embodiments, proper depth is in the scope of 1-4 centimetre (cm).Particulate is filled with subsequently, for example, and by the vibra-pack device.Then, the effect of filling is by the introscope vision-based detection.The base of filling is injected into cement subsequently.In one embodiment, cement is injected in the base under pressure.By shaking, rap and/or vibrating base, up to when observing with introscope, bubble stops at till the surface formation of base, thereby bubble is discharged base.Other then particle matter is added to the top of injecting base, repeats aforementioned process needs length up to formation cement.Cement can hardening, and solidifies under the temperature that improves.
Proper curing temperature can be determined by two factors: ability and (2) that (1) removes moisture from cement prevent the too high interior pressure that may cause breaking in the heater.Appropriate curing time can 1 hour to the scope in 2 weeks, this time is depended on the size of heater.Finishing of solidification process can be by a kind of judgement in the several method.In one embodiment, when the resistance by cement during, think that solidification process finishes greater than 100 kilohms (k Ω).In another embodiment, then be greater than 1 megaohm (M Ω).In another embodiment,, so that can and not be higher than at least 1 kilovolt (KV) and carry out the direct current high potential under 0.1 milliampere (mA) and test, think that then solidification process finishes when the resistance by cement is enough high.In one embodiment,, so that can and not be higher than at 0.5KV at least and carry out the direct current high potential under the 0.1mA and test, think that then solidification process finishes when the resistance by cement is enough high.In direct current high potential experiment, when interelectrode electric current was flow through in detection, the direct voltage between two electrodes increased progressively gradually.In this case, the heating element and first and/or second pipe can be selected as experimental electrode.If voltage surpasses certain threshold value, 1KV for example, electric current surpasses set-point simultaneously, and for example 0.1mA shows the stable high resistance of maintenances under high voltage, thinks that then it is successful testing.In another embodiment, do not separate out moisture, then think to solidify and finish when detecting by the dew point measuring appliance.In yet another embodiment, assert that according to mass loss curing finishes.For example, by earlier before the oven dry quality of heater deduct the quality of oven dry post-heater, from the quality of the water that is added with cement, deduct above-mentioned difference then, can calculate the quality of the water in the cement that remains in hardening.Like this, can record the wet quality of heater, and solidification process can continue the quality of the excessive water that the quality that reduces up to device equals to calculate.
In certain embodiments, heater comprises a plurality of heating elements, thereby each heating element is cooperated mutually and defined a plurality of Controllable Temperature thermal treatment zone or hot-zone.Each heating element comprises one or more electrical lead.In one embodiment, the heating element that defines each thermal treatment zone reel to form, thereby the two ends of same heating element or two lead-in wires stretch out from the independent end of this structure.In a heater embodiment with two Controllable Temperature thermals treatment zone, the two ends of heating element or two lead-in wires can stretch out from the relative two ends of heater.Have among the embodiment of two Controllable Temperature thermals treatment zone at another, the two ends of heating element or two lead-in wires stretch out from same end.In the embodiment that has more than two hot-zones, heating element end or lead-in wire can stretch out from shell, from an end, stretch out from arbitrary end or from the lip-deep difference along second pipe towards the outside.
The power density of heater can some key elements decide by controlling like this, for example rolling density or coiling pitch, and the selection of materials used in the heating element, the partial cross-section of heating element is long-pending, or the like.In one embodiment, the rolling density of heating element is consistent relatively, and variable quantity is less than about 25%.In another embodiment, the variable quantity of rolling density is less than about 10%.In one embodiment, the some parts of heater has higher rolling density with respect to other parts.In one embodiment, the end of heater has higher relatively rolling density with respect to the middle part of heater.The compensation end thermal loss speed higher with respect to zone between the end has been considered in the control of power density.In one embodiment, Temperature Distribution is consistent along the heater length direction.In one embodiment, rolling density defines from the gradient of the end to end of heater, thereby defines the Temperature Distribution pattern.In one embodiment, in two or more axially spaced hot-zones, temperature is relatively more consistent, and temperature has level and smooth transition between adjacent area.In certain embodiments, in the high-pressure crystal growing process, select pitch to prevent, to minimize or to eliminate the wall nucleation.
The example of suitable stratie comprises one or more in wire, band, coil, metal forming or the rod.One or more straties are reeled around central shaft in annular space.The heating element and the first pipe hot link, and electric insulation with it.Coiling can be thread-shaped, spirality or dual spirality.Some embodiment comprise triple or higher heavy corkscrews.Spiral wound makes the two ends of heating element stretch out from the same end of shell.Dual spiral makes the end of two independent heating elements stretch out from the same end of shell.The multiple coiling of a plurality of heating elements allows the Region control of heating element, here this is further specified.In one embodiment, the cross-sectional area of heating element is constant along its length direction.In another embodiment, the cross-sectional area of heating element changes along its length direction.The increase of the cross-sectional area of a sections of heating element will reduce the heating power density of this sections.By using dual or multi-spiral coiling heating element, the variation of element localized heating power density is useful.For example, the electric current that is added to first heating element mainly is applied to heating power first thermal treatment zone, and the electric current that is added to second heating element mainly is applied to heating power second thermal treatment zone, even two heating elements all are present in the zone of at least one form for reel dual spiral or multi-spiral.Having the long-pending heater sections of varying cross-section is connected by welding, brazing, crimping, clamping or similar approach.In another embodiment, by reversing or one or more other sections wiry being electrically connected with first sections wiry, the cross-sectional area of this heater sections part increases.
In one embodiment, heating element comprises the resistance heating wire of being made by KANTHAL A-1.Heating element is wound on first metal tube, is arranged to thus and the first pipe thermal communication.In one embodiment, electric insulation coating layer and/or at least one ceramic rod, ceramic particle filler or cement can be applicable on the heating element, thereby with the heating element and the first pipe electric insulation.Electric insulation coating layer and/or at least one ceramic rod, pottery tube, ceramic particle filler or cement also can be used for each heating element is electrically insulated from each other, and selectively, with the heating element and the first pipe electric insulation.In one embodiment, heating element by
Figure S06164789220070130D000071
The wire of making constitutes.
The example of suitable electric insulation coating layer comprises ceramic material, for example magnesium oxide.In one embodiment, electric insulation coating layer is a sandwich construction.In another embodiment, sandwich construction has the composition that is different from linearity or non-linear form along its thickness direction, thereby define a concentration gradient, for example, separate by the mixture of one deck YSZ and aluminium oxide between one or more layers yittrium oxide-stabilizing zirconia (YSZ) and the aluminium oxide.Further, sandwich construction can comprise one or more layers YSZ, aluminium oxide and/or their mixture.Layer structure can comprise ceramic insulating material, and described material is for example formed by plasma spraying deposition or electro beam physics steam deposition.The suitable component of ceramic rod is an aluminium oxide.When same ceramic particle filler and/or cement were used to fill annular space between first and second pipes, they can be used in provided electric insulation and thermal communication.
In one embodiment, stretch out in the one or more notch or the holes of cutting in second metal tube or the end ring of being passed in from heater in heating element, heating element end or the electrical lead.At heating element, end or the lead-in wire of extended position, by the electric insulation object, can insulate with the conductivity earth fault place of for example first pipe, and their also insulation each other.In one embodiment, the electric insulation object comprises aluminium oxide fabric or glass fibre tubulose fabric.In another embodiment, the electric insulation object comprises one or more snippets pottery or glass bushing.In yet another embodiment, the electric insulation object comprises pottery or bead.After heater was placed in the annular space, end ring can be fixed or be connected the end of heater.
With reference to Fig. 1-2 the specific examples of heater 100 is described, described heater comprises according to one or more specific embodiments of the present invention.As shown in the figure, second pipe 102 has inner surface, and this inner surface defines a space, and first pipe 104 is nested in the described space coaxially along axis 106.Second pipe internal surface and first pipe, 104 outer surfaces are spaced apart, thereby define therebetween microscler doughnut, annular space or slit.The arrow of mark " up " is represented direction upwards.Pipe 102,104 has first end 108, and axially spaced with first end and relative first second end of bringing in up 110.Therefore, word " top " expression second end is unless other meanings represented in context.
First stratie 111, second stratie 112 and the 3rd stratie 113 are set in the annular space.Among the embodiment, heating element is reeled twist as shown in the figure.Coil is represented its pitch to the 3rd stratie with Reference numeral 114 by reeling distance or pitch is apart opens.First and second straties extend different distances each other in the axial direction, thereby allow in use to regulate more accurately Temperature Distribution.First and second straties all are dual spirals, make two lead-in wires of each heating element all stretch out from the same end of heater.To the 3rd stratie, only shown a lead-in wire, that root lead-in wire that does not show may for example stretch out from the side of heater.
In illustrated embodiment, heating element comprises 18-specification wire, thereby can work under maximum 208 volts and 4000 watts.The electrical lead 115 that is used for the 3rd stratie stretches out from the bottom of heater.Other electrical lead that is used for other heating element does not show.Relative heating element, the thicker cross section that goes between has reduced resistance and the heat relevant with resistance.In one embodiment, form wire bundle by the wire that contacts other length at the lead-in wire outer surface, thus the thickness that is increased relatively.Wire bundle can be twisted into one, avoids in use can producing knot, pimple of local electrical resistance and relevant heat etc. simultaneously.In another embodiment, lead-in wire is folded back with self overlapping, thereby increases tranverse sectional thickness.
First pipe is coated with nonconducting ceramic coating.The ceramic coating of electric insulation is with the heating element sections and at least the first pipe electric insulation.In the illustrated embodiment, coating is a multi-layer compound structure.Composite construction comprises yittrium oxide-stabilizing zirconia (YSZ) and alumina layer, and they are separated by the different mixtures of multilayer YSZ and aluminium oxide.
Annular space or slit are filled up by the packing material 116 of high density and high alumina content.Be the packing material of cement in one embodiment, being in operation is pressed onto second pipe in first pipe outwards transmits, thereby makes heater storage variation/minimizing deformation and allow heater to reuse.
Heating element and first is managed thermal communication, and keeps electric insulation with first pipe and the second pipe both.Begin downward work from the top, the layout of a few cover heating elements defines several thermals treatment zone.The thermal treatment zone comprises uppermost first district 120, vitellarium 122, dividing plate slit region 124 and charging zone 126.When a container is inserted in the volume that is limited by first pipe internal surface 118, the internal partition (not shown) is aimed at the dividing plate slit region.Dividing plate defines two chambers in the container, and one is used to charge one and is used for growth.Two chambers are connected by dividing plate with holes.First pipe internal surface 118 may have one or more in the characteristic that further will discuss, particularly about the release characteristics of removable container.
In one embodiment, being fit to be inserted into first container of managing in 104 is formed by noble metal.The example of noble metal comprises platinum, gold or silver-colored.Other metals can comprise titanium, rhenium, copper, stainless steel, zirconium, tantalum and their alloy etc.In one embodiment, the function of these metals is equivalent to oxygen inhaler.The suitable dimension of container can be diameter greater than 2cm, length is 4cm.In one embodiment, diameter dimension can be selected in following scope: 2-4cm, and 4-8cm, 8-12cm, 12-16cm, 16-20cm, 20-24cm, and greater than 24cm.In second embodiment, the ratio of container length and diameter is greater than 2.In yet another embodiment, in the arbitrary below scope of the ratio of length and diameter: 2~4,4~6,6~8,8~9,9~10,10~11,11~12,12~14,14~16,16~18,18~20 and greater than 20.
In one embodiment, the volume of vitellarium 122 is twices of the volume of charging zone 126.The circuit of each heating element sections all is control separately.Separately control provides and has obtained and keep along the flexibility of the heat deposition distribution map of container height.The physics that the second and the 3rd heater sections begins from the top is discontinuous, has caused the part of the temperature at close dividing plate place to descend, and this dividing plate is arranged in the container and with charging zone 126 and vitellarium 122 to be separated.In one embodiment, charging zone and vitellarium are between isothermal region, but temperature is inequality each other.On the small distance between charging zone and the vitellarium thermoisopleth, baffle region has temperature gradient.The winding method of heating element, and consequent thermoisopleth with minimum temperature gradient interval have minimized or have eliminated the wall nucleation in the container.In one embodiment, the vitellarium can be in the bottom, and charging zone is on the top.This formation may be based on special chemistry and growth parameter(s).
(not shown) in another embodiment, heater have only a pipe (first pipe 104).In the manufacturing process of heater, second pipe is arranged on the outside of first pipe coaxially, and forms the annular space that will be full of packing material.After packing material curing partially or completely, remove second pipe by the known method of prior art, therefore second pipe does not become the part of making good heater.In one embodiment, second pipe is removed with mechanical means by grinding.In second embodiment, second pipe is chemically removed by dissolving.After removing second pipe, carry out the final curing of packing material.Have among the embodiment of heater (not shown) of single tube at another, first pipe is inserted in the mould, wherein forms cylindrical shape, polygon or the erose annular space that will be full of packing material between the inner surface of the outer surface of pipe and mould.Mould can be a porous, in the solidification process of packing material, allows moisture and other gaseous matters to overflow from annular space, shortens curing time thus and improves the consistency of curing filler material.Mould can comprise one or more parts, and can be after packing material curing partially or completely, by dismantle, break, method such as grinding is removed.The last curing of packing material can be carried out after removing mould.
With reference to figure 2, heater 100 is arranged in the device 200 that includes container 210 especially.This container head is connected with first end cap 212, and the bottom is connected with second end cap 214.A plurality of securing members 216 (having only one of them to be expressed by Reference numeral) are fixed on container ends with end cap.
In container 210, pressure transmission medium 230 is packed in inner surface of container and contacts with the outer surface of heater 100.The example of pressure transmission medium is including, but not limited to zirconia.First and second pressure transmission mediums lid 232 (only one of them is shown) closely is arranged on the place, end of container internal heater 100.Ring plug 234 is shown as the disk of stack, but can be around covering 232 annulus.Selectively, stopper 234 can be set at least one end, and in the cavity between heater end and end ring, thereby reduce axial heat loss.Stopper can buy by different channels, comprises Thermal CeramicsWorldwide (Augusta, Georgia), and trade mark is KAOWOOL.
In the illustrated embodiment,
Figure S06164789220070130D000101
Heating element 112 is embedded in the packing material 116.The pressure transmission medium layer is provided with around heater 100, and the end holds stopper.Selectable stopper material can comprise magnesium oxide, magnesium salts, phyllosilicate mineral matter, for example hydroxide sial or pyrophyllite.
Graphic display unit 200 can be used for grown crystal under the pressure and temperature that is fit to crystal growth, for example, and the gallium nitride under associated process conditions.High-pressure installation 200 can comprise one or more can be radially, axially or support the structure of heater 100 simultaneously radial and axially.In one embodiment, supporting construction is isolated device 200 and surrounding environment heat, and this heat insulation stability that can improve or improve process, keeps and control the desired temperatures distribution map.
Referring to Fig. 3, shown the cross section top view of another heater embodiment 300.Heater 300 comprises first pipe 302 and the heating component 304.Heating component can have different shape of cross sections, the shape of a hoof and oval cross section shown in Reference numeral 305,306 difference.First pipe has shell or outer surface 308, and it defines at least one groove or passage 310.Each heating component (304,305 and 306) all include second outer tube 320, middle heating element 322 and be arranged on second the pipe and heating element between electric insulation ceramics filler 324.In order clearly to illustrate, be not arranged on heating component wherein in the groove that is labeled.According to embodiments of the invention, the groove of different depth or passage can use in identical or different heater.In addition, the groove with different openings width can be used.For example, the A/F of opening 316 is narrower relatively than the A/F of another opening 318.The spatial radial that limits when groove or passage moves inward, and when keeping curvilinear sidewall simultaneously, in one embodiment, A/F reduces.If A/F is reduced to less than the width of heating element, heating element (or second pipe) can be from end axis for example to insertion so.In alternate embodiments, width can reduce to zero.
Heating component 304 is nestedly packed in the groove 310.Heating component 304 can be the CALROD heating component.Heating component 304 comprise optional second outer tube 320, middle heating component 322 and be arranged on first the pipe and heating element between electric insulation ceramics filler 324.
Manage and have the heater of ceramic filler on every side by rocking second downwards, can remove or minimize remaining space or hole between the heating element and second pipe, thus constituent components.Passage or groove 310 are adapted to the shape of heating component 304.Before embedding heating element, groove surfaces can be machined, mills or polish, thus the thermal communication that smooth, polished, close tolerance is provided and strengthens.Groove can have spiral shape, and heating component bends to spiral shape so that be fit to groove, thereby one or more heating component can be used, to be provided at the inner uniform heating of first pipe.
In the illustrated embodiment with heater assembly 305, in the space between first tube-surface 308 and heating component 305 outer surfaces, be full of ceramic material 328 in the groove 310, it can or conduction or electric insulation.Some embodiment can be included in the extra grafting material of interpolation of corner.These extra cements are used for surrounding the corner, thereby improve the integrality of heat and/or structure.
In another embodiment of the heater assembly that does not have second pipe, assembly comprises the heating element 322 that is arranged in groove or the passage 310 interior spaces.Packing material (cement) is disposed between the heating element 322 and first tube-surface 308.Packing material can foregoingly be cured.In example, packing material conducts electricity therein, and the electrical insulating material that heating element 322 is at first had enough dielectric strengths applies.
In another embodiment, be different from grafting material, the remaining space in the groove can be full of and the first pipe identical materials.The pipe packing material can obtain by method electrochemical depositions such as powder metallurgy, physical vapor deposition, chemical vapour depositions.
In one embodiment, heater can comprise a plurality of different heating elements, limits the hot-zone that two, three or more temperature can control.Shown in the assembly 400 of Fig. 4, can hold a plurality of hot-zones.First pipe 402 is coated with first dielectric ceramic layer 404.Controller 406 imports into and outgoing signal to a plurality of heating element sections 410,412,414,416, and these heating element sections are centered around in forming process outside first pipe of heat conduction and electric insulation, is made up of part or a plurality of coiling coil.Also there is shared sections 418, to finish the loop.Extra dielectric ceramic layer (not shown) can be placed on one or more heating element sections, makes the lead-in wire electric insulation of they and controller 406.One or more electrical pickofves can be used to connect the end of each heating element sections.
Electrical pickoff can be made of relative material and/or the more low-resistance material than the weight-normality lattice, thus the preferentially generation rather than in electrical lead in the heating element sections of most of heating degree.Electrical lead can be by spot welding, arc-welding, ultrasonic bonding, brazing, connect securing member, screw clamp etc. fast is connected on the heater sections.One or more additional ceramic coatings can reduce or eliminate the short circuit of electrical lead and other heater sections.The ceramic grafting material (not shown) that can cast can be packed into or be cast on the above-mentioned assembly.Second pipe can be placed on the assembly, thereby finishes a heater according to the embodiment of the invention.
Controller 406 communicates with the transducer (not shown), and with heating element 410,412,414,416 communicate.Right sensors comprises temperature sensor and/or the pressure sensor that is positioned at the detected district of next-door neighbour.In one embodiment, temperature sensor is made up of thermocouple.The existence in a plurality of districts has been considered by the desired temperature distribution controlled quentity controlled variable in the heater 400 of controller 406, thereby has finally been controlled first pipe 104 and/or the interior heat distribution of reaction vessel (if there is).In addition, the electrical power of each sections can be designed to the function of time, and controller can be handled the Temperature Distribution in the heater 400 like this.The control of this Temperature Distribution is of value to the diversity of growing method, for example the hydro-thermal growing method.
In an embodiment of crystal growing process, the energy that offers heating element causes heat energy to flow into first pipe entering the container that is arranged in the territory, first area under control.The heat that provides makes the temperature of container be elevated to temperature range greater than 500 ℃, and as the response that temperature is raise, can be enough in container generation greater than the pressure of 500MPa.In operation, packing material outwards transmits internal pressure to the second pipe from first pipe, thereby makes heater storage change/minimizing deformation.Because packing material is incompressible fully, therefore help to keep the volume and/or the shape of heater.Be fixed among the embodiment of end ring of first end of pipe in utilization, the volume and/or the shape of heater can be fixed further in operation.
If the volume minimally of first pipe changes, and the distortion of its shape minimally, heater can be reused under high pressure-temperature operation subsequently so.In one embodiment, the change of the internal capacity of first pipe (inside and two ends by first pipe limit) is less than 10vol.%.In second embodiment, first pipe causes that the internal capacity less than 5% changes.In the 3rd embodiment, volume-variation is less than 2%.In one embodiment, the change of the external volume of first pipe (internal capacity by shell limits) is less than 10vol.%.In second embodiment, first pipe causes that the external volume less than 5% changes.In the 3rd embodiment, external volume changes less than 2%.Because inside (first) pipe of heater causes minimum volume-variation, and stand seldom or the slit that does not have, crack or be interrupted, therefore be arranged on the container in the heater that is operated in the high pressure/high temperature environment, after operation is finished, can from heater, shift out slidably.Here " to shift out " meaning slidably be that container can skid off from the inner surface of first pipe to the word of Shi Yonging, and need not to use too much strength, also can not produce permanent infringement to heater.In one embodiment, container is at one end gone up by hydraulic pressure and is loaded, and for example by the use hydraulic piston, thereby skids off from the inside of first pipe.Move in order to prevent that heater from transmitting the material from pressure, the constraint of machinery can be provided.After beginning operation, after container shifted out from first pipe slidably, heater can also be reused repeatedly.
Embodiment described here is the example of composition, structure, system and method, the key element that the key element that they have is stated in the claims corresponding to the present invention.These written explanations make those of ordinary skills can make and use the embodiment with alternative key element, the key element that described key element is similarly stated in claims corresponding to the present invention.Therefore, described scope comprises composition, structure, the system and method as broad as long with the claim literal language, and comprises that further literal language with claims does not have other compositions, structure, the system and method for substantive difference.Although only illustrate and described some feature and embodiment, concerning the person of ordinary skill in the relevant, can be easy to expect many modifications and change here.Claim is used for covering all such modification and changes.

Claims (23)

1. heater that in high-pressure and high-temperature device, uses, this heater comprises:
Define first pipe of axis, this pipe has first end and second end, and second end and the first end axially-spaced, and this pipe has outer surface and inner surface, and inner surface can storage container;
Packing material, be set near or be close to the outer surface of this pipe;
One or more heating elements, itself and this pipe thermal communication and being at least partially disposed in this packing material;
Wherein, in response in this device greater than the operating pressure of 150MPa with greater than 200 ℃ temperature, the volume of this packing material reduces less than 5 percents by volume, allows this container is shifted out from first pipe slidably.
2. heater as claimed in claim 1 is characterized in that, described heater comprises that also being arranged on second outside first pipe manages, and this packing material is arranged between first pipe and second pipe.
3. heater as claimed in claim 2, it is characterized in that, described first pipe is in coaxial relation with second pipe or shell, and first pipe has inner surface and outer surface, radially separate between described inner surface and the axis, thereby limit the volume that is large enough to hold reaction vessel, the inner surface of the described outer surface and second pipe radially separates, and making is enough to limit a slit; With
Packing material is arranged in this slit.
4. as each described heater among the claim 2-3, it is characterized in that the packing material that is in operation can be operable to second pipe is transmitted and passed to the internal pressure of first pipe radially outwardly.
5. as each described heater among the claim 2-3, it is characterized in that, make heating element and first pipe, or simultaneously and first pipe and the second pipe electric insulation with second pipe by one deck electric insulation layer at least.
6. heater as claimed in claim 5 is characterized in that electric insulation layer comprises the electric insulation ceramics material, and this material is selected from yittrium oxide-stabilizing zirconia, aluminium oxide or its composition.
7. heater as claimed in claim 5 is characterized in that, electric insulation layer is a multilayer, and the coating of this multilayer has every layer of different composition, thereby defines a component gradient along the thickness of electric insulation layer.
8. as each described heater among the claim 2-3, it is characterized in that, described heater also comprises the one or more electrical insulating materials that are arranged in the packing material, this electrical insulating material can make at least one and first pipe in the heating element, with second pipe, simultaneously with first pipe and second pipe or with other heating elements insulation.
9. as each described heater among the claim 2-3, it is characterized in that described heater also comprises first end ring, this first end ring be fixed on first pipe first end, second pipe first end or be fixed on simultaneously on first end of first pipe and second pipe.
10. as each described heater among the claim 1-3, it is characterized in that the outer surface of first pipe defines passage or groove, and in these one or more heating elements at least one is included in the assembly that is at least partially disposed in this passage or the groove.
11. as each described heater among the claim 1-3, it is characterized in that, reaction vessel can hold and preserve medium, this medium to become postcritical mode in response to heat and pressure, and reaction vessel is positioned in first pipe in operation, the internal capacity of first pipe is configured to define constant volume, to allow in response to temperature build-up pressure in reaction vessel, so that make the temperature and pressure enough height and to make medium be postcritical all in the reaction vessel in operation, the required pressure of supercriticality is provided by the restriction to volume, and the described restricted passage inner surface of first pipe of defined reaction container outer surface passively provides.
12. be used for the heater assembly of high-pressure and high-temperature device, comprise:
First pipe with inner surface and outer surface, but inner surface defines the chamber that is configured to storage container, and outer surface defines at least one groove or passage;
Be arranged on the packing material in groove or the passage, at least one heating element is arranged in this packing material, and this heating element is logical with the first pipe hot link by this packing material, and with first manage electric insulation;
Wherein, in response in this device greater than the operating pressure of 150MPa with greater than 200 ℃ temperature, the volume of this packing material reduces less than 5 percents by volume, allows this container is shifted out from first pipe slidably.
13. heater assembly as claimed in claim 12 is characterized in that, described heater assembly also comprises non-conductive ceramic coating, and this coating contacts with the outer surface of heating element and the inner surface of groove or passage.
14. as each described heater assembly among the claim 12-13, it is characterized in that, described heater assembly comprises that also at least one is arranged on second pipe in passage or the groove, packing material is arranged in second pipe, heating element is arranged in second pipe, and by the packing material and the second pipe electric insulation.
15. heater assembly as claimed in claim 14 is characterized in that, described heater assembly also comprises cement conduction or electric insulation, and it is arranged in groove or the passage and outside second pipe, and second pipe and groove or passage are separated.
16. a heater assembly comprises:
Heating element can be operable to the temperature range that is heated to greater than 500 ℃;
Surround the cement charges of this heating element, these cement charges have first surface and opposing second surface;
First pipe and second pipe, wherein first pipe communicates with the first surface of these cement charges and for it provides mechanical support, and second manage and communicate with the second surface of these cement charges; And
In operation, the energy that offers this heating element causes heat energy to flow into first pipe, enter the container that is located in the territory, first area under control, this heat energy is enough to make the temperature of this container to be elevated to scope greater than 500 ℃, and the response that raises as temperature and in this container, being created in greater than the pressure in the 500MPa scope, simultaneously first pipe is limited by these cement charges, so that make amount that the volume in this container increases less than 5%.
17. heater assembly as claimed in claim 16 is characterized in that, the root mean square surface roughness of the inner surface of first pipe is less than 1 millimeter, and do not have size greater than 5 millimeters one or more slits, crack or interruption.
18. each described heater assembly among the claim 16-17, it is characterized in that, in response in this heater assembly greater than the operating pressure of 500MPa with greater than 500 ℃ temperature, the volume of packing material reduces less than 5 percents by volume, allows container is shifted out from first pipe slidably.
19. as each described heater assembly among the claim 16-17, it is characterized in that, packing material comprises cement that can cast or moldable, and this cement has greater than the resistance of 100 kilohms (k Ω) and is at least 75% density of theoretical maximum density.
20., it is characterized in that packing material comprises that quantity accounts for magnesium oxide, aluminium oxide or magnesium oxide and the aluminium oxide in 70 to 80 weight percentage ranges as each described heater assembly among the claim 16-17.
21., it is characterized in that greater than the pressure of 700MPa and under greater than 700 degrees centigrade temperature, the volume that packing material has less than 10% reduces as each described heater among the claim 16-17.
22., it is characterized in that heating element is a kind of in metal forming, band or the silk as each described heater assembly among the claim 16-17, and limit thread-shaped, snakelike, single-screw shape, dual spirality or multi-spiral shape.
23., it is characterized in that first end and second end of first pipe limit internal capacity as each described heater assembly among the claim 16-17, and wherein
In response in the heater assembly greater than the operating pressure of 500MPa with greater than 500 ℃ temperature, the volume of packing material reduces less than 5 percents by volume, and the variation of internal capacity allows container is shifted out from first pipe slidably less than 10 percents by volume.
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CN101146379A (en) 2008-03-19
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US20080083741A1 (en) 2008-04-10
EP1901584A2 (en) 2008-03-19
KR101310437B1 (en) 2013-09-25
EP1901584A3 (en) 2008-09-10
US7705276B2 (en) 2010-04-27
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PL1901584T3 (en) 2016-09-30
JP5044202B2 (en) 2012-10-10

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